反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
2-(Ethylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (120 mg) and iodomethane (37.8 μl) were dissolved in N,N-dimethylformamide (2 ml), sodium hydride (60% in oil, 86 mg) was added thereto under ice-cooling, and the mixture was stirred for 45 min. 0.5M Hydrochloric acid (6 ml) was added thereto under ice-cooling, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained white solid residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (123 mg) as a white solid.
WORKUP
后处理
- temperatureunder ice-cooling
- temperatureunder ice-cooling
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe obtained white solid residue was purified by silica gel column chromatography (ethyl acetate/hexane)